73 results about "N-butyl nitrite" patented technology

The invention discloses a synthesis method of a 1,2,3-diazosulfide compound. A o-aminothiophenol compound with a structure shown as a formula (I) and tert-butyl nitrite are taken as raw materials, and are subjected to intramolecular diazo-reaction to obtain the 1,2,3-diazosulfide compound with a structure shown as a formula (II); a reaction equation is as follows (shown in the description), wherein R=hydrogen, fluorine, chlorine, ester group, nitro or methyl. The synthesis method has the beneficial effects that (1) the operation is simple and convenient in a preparation process, an obtained product is easy for after-treatment, and large-scale industrialized production is suitable; (2) reaction conditions are mild; (3) the synthesis cost is lowered; (4) a reaction substrate is high in functional group tolerance, is wide in range and easy to prepare; (5) the reaction is efficient, the yield is high, and the reaction efficiency is higher after reaction amplification; (6) environment pollution is avoided, and environment friendliness is achieved.

The invention relates to benzotriazole compounds and a preparing method thereof. o-phenylenediamine or an o-phenylenediamine compound n-butyl nitrite are adopted as reaction raw materials and are subjected to an intramolecular diazo-reaction at room temperature in a reaction solvent to obtain the corresponding benzotriazole compound. According to the method, the range of substrates is wide, reaction conditions are mild, after-treatment is simple, and a product yield and quality are high. A novel synthesis route and method for the benzotriazole compounds are developed. The benzotriazole compounds have good application potentials and research value.

A disclosed preparation method for erythro-structure methoxamine hydrochloride comprises the following steps: (1) dissolving an initial raw material 2,5-dimethylpropiophenone in an organic solvent, under the condition of introducing dry hydrogen chloride gas, dropwise adding a 1-butyl nitrite solution to perform an oximation reaction, so as to obtain an intermediate I; (2) under the acidic condition, taking a methanol solution as a solvent, take palladium on activated carbon as a catalyst, employing hydrogen to reduce the oximido group in the intermediate I, so as to obtain an intermediate II; and (3) performing hydrogenation reduction reaction on the intermediate II to obtain the erythro-structure methoxamine hydrochloride. The method provided by the invention is simple in operation, economic, environment-friendly, mild in reaction conditions, excellent in product quality and high in yield, and can help to obtain the single erythro-structure methoxamine hydrochloride.

The invention relates to a hydrogen sulfide fluorescent probe as well as preparation and application thereof. The molecular formula of the fluorescent probe is C27H25NO9; the preparation method of thefluorescent probe comprises the following steps: reacting a fluorescein with sodium hydroxide; reacting an obtained product with 2-(2-(2-methoxyethoxy)ethoxy)ethyl 4-methylbenzenesulfonate to obtaina compound 4, reacting the compound 4 with N-Phenylbis(trifluoromethanesulphonimide) to obtain a compound 3, reacting the compound 3 with bis (pinacolato) diboron to obtain a compound 2, hydrolyzing the compound 2, and reacting an obtained product with tert-butyl nitrite to obtain the hydrogen sulfide fluorescent probe. The probe shows relatively high selectivity on detection of hydrogen sulfide in a pure water solution.

The invention provides a method for preparing a chiral 3-nitroindole compound through a nickel-catalyzed asymmetric nitration reaction. The method comprises the following steps: in a solvent, under the action of an additive, a nickel catalyst and a ligand, carrying out an asymmetric nitration reaction on an indole-2-one compound I and tert-butyl nitrite II to obtain the chiral 3-nitroindole compound III. According to the invention, chiral 3-nitroindole is constructed through a nickel-catalyzed asymmetric nitration reaction, and the method has the advantages of low catalyst cost, convenience in operation, wide substrate application range, cheap and easily available reaction raw materials and the like.

The invention discloses a synthesis method of a 1,2,3-phentriazine-4(3H)-one compound. 2-aminobenzamide and are used as raw materials and tert-butyl nitrite stirred at the room temperature in a reaction solvent, and the 1,2,3-phentriazine-4(3H)-one compound is obtained through an intramolecular diazotization reaction. The reaction equation is shown in the description, wherein R is H, fluorine, chlorine, bromine, trifluoromethyl, nitryl or methyl. The synthesis method has the benefits as follows: (1) the synthesis method is convenient in experiment operation, easy in posttreatment, mild in reaction condition and suitable of large-scale industrial production; (2) reaction substrate functional groups have high tolerance, and the substrate is wide in range and easy to obtain; (3) the reactionefficiency, yield and purity are higher.

The invention belongs to the technical field of medicine synthesis, and in particular relates to a method for synthesizing a Crizotinib intermediate. The method comprises steps of: a) reacting a raw material 4-mesylate piperidine-1-formic acid tert-butyl ester (2) with 4-nitro pyrazole to prepare a compound 3; b) reducing nitro by using hydrazine hydrate to obtain an amino compound 4; and c) diazotizing the compound 4 by using tert-butyl nitrite, and reacting the compound 4 with a boric acid ester compound 5 in the presence of a free radical initiator benzoyl peroxide, so as to prepare the Crizotinib intermediate (1). Compared with an existing synthesis method, the method provided by the invention has the following advantages: a diazotization method is used to synthesize the boric acid ester product; and compared with an existing Miyaura boronation method catalyzed by Pd, the method avoids the usage of expensive palladium catalyst and ligand, and has the merits of mild reaction condition, high yield, simple operation, cheap and easily available raw materials and short reaction period, and is quite easy for industrialized mass production.

The invention discloses a simple preparation method of isoxazoline. The simple preparation method is characterized in that a series of isoxazoline compounds are efficiently synthesized by using aldehyde, p-toluenesulfonhydrazide, olefin and tert-butyl nitrite as substrates, copper chloride as a catalyst and tetramethylethylenediamine (TMEDA) as alkali through the one-pot two-step method. The method has the advantages that the catalyst is cheap, reaction is economical, good substrate universality is achieved, the raw materials are easy to obtain, later-stage functionalization is more convenient, reaction conditions are mild, and gram-level scale reaction is good; and especially, the compounds with medium yield can be obtained without the catalyst, post-treatment is simple and convenient, the application of the compoumds in drug molecule synthesis and large-scale industrialization is facilitated, and the requirements and trends of modern green chemistry and medicinal chemistry are met.

The invention relates to the technical field of synthetic rubber, and discloses rubber containing modified graphene, which comprises the following components: rubber, carbon black, zinc oxide, stearic acid, sulfur, an accelerant, a scorch retarder and modified graphene. The modified graphene is obtained by fully mixing and ball-milling graphite and a modifier, then adding tert-butyl nitrite and a solvent, mixing and ball-milling, fully mixing, washing and drying; and the modifying agent is one or more of amino propionyl aniline, 4-aminobenzoyl aniline, 2-amino-N-cyclohexyl-N-methyl benzene methylamine, 4-(4-isopropyl piperazine-1-yl) aniline, (4-aminobenzene)-4-(4-methoxyphenyl) piperazine, (4-(4-aminobenzyl) piperazine-1-yl) ethanone and (4-aminobenzene)-4-(4-methoxyphenyl) piperazine. Rubber formed by mixing and refining the modified graphene and other components of rubber has a better anti-aging effect.

The invention belongs to the field of organic synthesis and azo dyes and particularly discloses an imidazo heterocyclic azo derivative and a preparation method and application thereof. The imidazo heterocyclic azo derivative has a structural formula shown as in formula (1), wherein heterocyclic Het is one of pyridine, thiazole and pyrimidine; R is C1-C6 alkyl groups, or aryl groups containing F, Cl, Br, MeO, CN and NO2 or aryl groups that are acetyl-substituted; Ar is aryl groups containing F, Cl, Br, MeO, CN and NO2 or aryl groups that are acetyl-substituted. The preparation method of the invention is an economical, simple and environment-friendly green synthetic method, neither the addition of mass hydrochloric acid or sulfuric acid and nitrites nor the pre-preparation of diazonium salts is required in the method, and imidazo heterocyclic azo compounds are directly produced under the action of tert-butyl nitrites. The imidazo heterocyclic azo derivative prepared herein has good fluorescent properties and is useful in the fields such as fluorescent dyes, luminescent materials and bactericides.

The invention discloses a preparation method of 1-(tert-butyl)-3-chloronaphthalene. The preparation method comprises the following steps: reacting 1-naphthylamine with N-chlorosuccinimide in a solvent to generate a first intermediate; reacting the first intermediate with N-bromosuccinimide in a solvent to generate a second intermediate; reacting a first reaction system containing the second intermediate, lewis acid, tert-butyl nitrite and a solvent, and then adding hypophosphorous acid and cuprous oxide into the first reaction system for reaction to generate a third intermediate; and reacting a second reaction system containing a catalyst ligand, nickel acetylacetonate, lithium tert-butoxide, isopropyl magnesium chloride and a solvent in a protective atmosphere, and then adding the third intermediate into the second reaction system for reaction to generate 1-(tert-butyl)-3-chloronaphthalene. The preparation method disclosed by the invention is short in process route, simple to operate, mild in condition, environment-friendly, low in cost, high in target product yield, few in by-products and beneficial to industrial production.

The invention discloses a synthesis method of 2-(2-methoxy-4-nitrophenyl)-3-(4-nitrophenyl)-5-(2,4-disulfophenyl)-2H-tetrazole monosodium salt (WST-8), belonging to the technical field of chemical synthesis. According to the synthesis method, the raw materials benzaldehyde-2,4-sodium disulfonate and p-nitrophenylhydrazine are subjected to four-step reaction by using N-bromosuccinimide (NBS) as an oxidizer, thereby obtaining the WST-8. The invention is safe and simple to operate and easy for after-treatment, and avoids using chlorine gas, n-butyl nitrite and other high-toxicity high-price compounds; and the total yield of the four-step reaction is up to 34.4%, thereby being beneficial to industrial production.

The invention discloses a chromium-containing waste leather scrap treatment method. The method comprises the following steps: carrying out hydrolysis treatment on chromium-containing waste leather scraps serving as a raw material, and carrying out enzyme hydrolysis on the chromium-containing waste leather scraps by using protease; carrying out further hydrolysis on the chromium-containing waste leather scraps by using an acid solution to hydrolyze the chromium-containing waste scraps into collagen polypeptide molecules, wherein the acid solution is a mixture of an aqueous sulfuric acid solution and an aqueous lactic acid solution; then modifying the collagen polypeptide molecules with a modifier, wherein the modifier is consisting mixture of of 2,3-pyridinedioic anhydride, 7-chloro-2H-benzo[e][1,2,3,4]thiatriazine-1,1-dioxide and 4,4'-diamino-3,3'-biphenyl disulfonic acid, wherein the 7-chloro-2H-benzo[e][1,2,3,4]thiatriazine-1,1-dioxide is obtained by reacting 2-amino-5-chlorobenzenesulfonamide with tert-butyl nitrite; and performing treatment to process the chromium-containing waste leather scraps into a retanning filler. The retanning filler has a good tanning and retanning filling effect, and tanned leather is full, soft, good in elasticity and clear and fine in grain.

The invention discloses a method for synthesizing an aromatic trifluoromethylthio compound. The method comprises the following steps: reacting sodium trifluoromethanesulfinate with Chlorodiphenyl phosphine at room temperature; after reacting for a period of time, sequentially adding an aniline compound and tert-butyl nitrite, fully reacting at 70 +/-5 DEG C by taking CuSO4 as a catalyst and acetonitrile as a solvent, cooling to room temperature after the reaction is finished, extracting, carrying out reduced pressure distillation, and carrying out column chromatography separation and purification on the reaction mixture to obtain the aromatic trifluoromethylthio compound. The method is simple and safe in process operation and high in reaction conversion rate, the used raw materials are economical and practical, few three wastes are generated, and no extra organic solvent needs to be treated.